An automated inline sample preparation (ILSP) method has been developed for pesticide residue analysis in spinach by LC-MS/MS. Chlorophyll pigments and other matrix constituents were removed from the sample extract using a UHPLC system equipped with an auxiliary pump, 6-port high pressure switching valve, and dual-directional ILSP cartridge containing bonded silica. The new procedure was evaluated as an entirely separate workflow using a simple solid-liquid extraction and as part of a cleanup strategy in conjunction with QuEChERS. Accuracy and precision experiments were conducted in spinach at two concentration levels (n = 6). Of the 63 pesticides tested, 86% (0.005 mg/kg) and 100% (0.05 mg/kg) displayed average recoveries within 70–120% and RSD values ≤20% for the ILSP method. In addition, low to moderate matrix effects (<50%) were calculated for 95% of the analytes. Overall performance of the proposed method was found to be better or comparable to a traditional QuEChERS procedure utilizing AOAC formulated salts and dSPE sorbents, while significantly reducing the amount of pigments reaching the MS source. The ILSP workflow is a simpler procedure with fewer steps that require less time than traditional extraction and cleanup techniques.

已经开发了一种自动在线样品制备（ILSP）方法，用于通过LC-MS / MS分析菠菜中的农药残留。使用配备了辅助泵，6通高压切换阀和包含键合硅胶的双向ILSP滤芯的UHPLC系统，从样品提取物中去除了叶绿素颜料和其他基质成分。该新程序使用简单的固液萃取方法作为完全独立的工作流程进行了评估，并与QuEChERS一起作为净化策略的一部分进行了评估。在菠菜中以两个浓度水平（n = 6）。在63种农药中，ILSP方法的86％（0.005 mg / kg）和100％（0.05 mg / kg）的平均回收率在70-120％之间，RSD值≤20％。此外，对于95％的分析物，计算出低至中等的基质效应（<50％）。发现所提出方法的总体性能优于或优于使用AOAC配制的盐和dSPE吸附剂的传统QuEChERS方法，同时显着减少了到达MS源的颜料量。与传统的提取和清除技术相比，IRLSP工作流是一个更简单的过程，所需的步骤更少。